试样用盐酸-硝酸溶解,采用反应池技术消除复合离子对Cr、Si元素的干扰,Pt对Au元素影响采用反应池技术与等效法扣除,以内标校正法直接测定其它 15 个元素.优化选择了测定同位素和内标元素,考察了基体效应对测定结果的影响,建立了电感耦合等离子体质谱(ICP-MS)法测定高纯铂中18个痕量杂质元素含量的方法.被测元素的检出限为0.0031~1.16 ng/mL,样品的加标回收率在85.7%~119.8%之间,相对标准偏差(RSD)为1.76%~4.50%.方法可以满足4~5 N高纯铂产品的测定要求.
The interferences for Cr, Si and Au produced by polyatomic ions were eliminated by reaction cell technology and the interference with minus equivalent concentration method. The other 15 impurities were determined directly by intemal standard correction method. The samples were dissolved in HCl-HNO3. Under the optimized conditions of measured isotopes and intemal standard elements, the matrix effects were investigated and the method for the analysis of 18 trace-impurities in high purity platinum was established. Determination limits obtained ranged 0.0031~1.16 ng/mL for 18 impurities. The recovery of standard addition was in the range of 85.7%~119.8%, and the relative standard deviation (RSD) was 1.76%~4.50%. The method can be used for the analysis of 4~5 N high purity platinum products.
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